HRID1603550

反应详情

EQUATION

反应方程式

HRID 1603550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.09 g (0.000275 mol) of (4-benzenesulphonyl-6-bromopyridin-2-yl)-methylamine was dissolved in 7 ml of ethanol, treated with 0.009 g of Pd/C (10%) and hydrogenated under normal pressure for 18 hrs. Thereafter, the catalyst was filtered off, the solvent was removed and the residue was partitioned in ethyl acetate and saturated bicarbonate solution. The organic phase was washed with sat. sodium chloride solution and dried over MgSO4. After removal of the solvent the residue was chromatographed on silica gel with ethyl acetate/hexane 1:4 and 1:3. There was obtained 0.025 g (37%) of (4-benzenesulphonylpyridin-2-yl)-methylamine as beige crystals; m.p.: 142-143° C.

WORKUP

后处理

  1. filtrationThereafter, the catalyst was filtered off
  2. customthe solvent was removed
  3. customthe residue was partitioned in ethyl acetate
  4. washThe organic phase was washed with sat. sodium chloride solution
  5. dry with materialdried over MgSO4
  6. customAfter removal of the solvent the residue
  7. customwas chromatographed on silica gel with ethyl acetate/hexane 1:4 and 1:3